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Method for purifying nitric oxide

A nitric oxide and refining method technology, applied in nitric oxide, chemical instruments and methods, separation methods, etc., can solve the problems of liquid nitric oxide explosion, expensive equipment, complex cooling operation, etc.

Active Publication Date: 2014-04-02
SUMITOMO SEIKA CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, the cooling operation using liquid nitrogen is complicated, the equipment is expensive, and there is a possibility of explosion of liquid nitrogen monoxide, so it cannot be said that it is suitable for industrialization.

Method used

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  • Method for purifying nitric oxide
  • Method for purifying nitric oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] In embodiment 1, omit above-mentioned implementation mode ( figure 1 ) in the absorbing liquid contact device 1 performs an adsorption process on the crude NO gas supplied from the NO cartridge Y1 with the adsorption tube 2 . Activated alumina (trade name: KHD-12, manufactured by Sumitomo Chemical Co., Ltd.) was used as the inorganic adsorbent filled in the adsorption tube 2 . As pretreatment of the adsorbent, 18.6 g of activated alumina and 0.3 N of nitric acid aqueous solution were mixed and stirred at 40° C. for 2 hours, and then vacuum-dried at 60° C. for 6 hours. The pretreated adsorbent obtained in this way is filled in the adsorption tube 2 (a stainless steel cylindrical adsorption tube with an inner diameter of 7.5 mm and a length of 500 mm. After that, the temperature of the adsorption tube 2 is raised to 150° C. and the on-off valves 4A to 4D are closed. state and the on-off valve 4E is in the open state, the vacuum pump 8 is operated, and the vacuum is carri...

Embodiment 2

[0049] In Example 2, molecular sieve 4A (trade name: Zeolum A-4, manufactured by Tosoh Corporation) was used instead of the activated alumina of Example 1 as the inorganic adsorbent. NO purification (pretreatment and adsorption steps) was carried out in the same manner as in Example 1 except that the inorganic adsorbent was changed. When 1 hour has elapsed after the flow of the raw material gas to the adsorption tube 2 has passed, the result of analyzing the non-adsorbed gas derived from the adsorption tube 2 is, H 2 O content = 1ppm, NO 2 Content=25ppm, N 2 O content = 60ppm, N before and after circulation 2 O content increment is 10ppm.

Embodiment 3

[0051] In Example 3, as pretreatment of the adsorbent, 150 ml of activated alumina (trade name: KHD-12, manufactured by Sumitomo Chemical Co., Ltd.) was placed in a stainless steel autoclave with an inner capacity of 300 ml and a pressure resistance of 3 MPa, and added NO / NO 2 =1 / 1 mixed gas up to 1.5MPaG. After 4 hours at 40°C, purge gas was introduced and NO / NO was added again 2 =1 / 1 mixed gas up to 1.5MPaG, keep at 30°C for 5 hours. The adsorbent thus pretreated was filled in the same adsorption tube 2 as in Example 1, and purified in the same manner as in Example 1 for supplying the raw material gas. When 1 hour has elapsed after the start of circulation, the result of analyzing the non-adsorbed gas derived from the adsorption tube 2 is, H 2 O content = 1ppm, NO 2 Content=30ppm, N 2 O content = 63ppm, N before and after circulation 2The O content increment was 13 ppm.

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Abstract

The present invention provides a refinement method and purification system of the suitable to obtain the nitrogen monoxide gas of the high purity. The nitrogen oxide suppressing the production of the by-product subject is solved. And the refinement method of the nitrogen oxide of the present invention includes at least nitrogen oxide, and the adsorption process for conducting the mixing gas containing moisture on the inorganic world absorbent and absorbing moisture in the corresponding absorber. And as the inorganic world absorbent, the preprocessing completion absorber in which the preprocessing for creating the inorganic acid salt is put into effect in advance is used. The invention the system for performing provides the refinement method of such nitrogen oxide.

Description

technical field [0001] The present invention relates to methods and systems for refining nitric oxide. Background technique [0002] Nitrogen monoxide can be used, for example, as a material gas for forming an oxynitride film (SiON film) on a silicon surface in a semiconductor process. Nitric oxide is produced by various methods such as the ammonia oxidation method, the method of reacting sodium nitrite and ferrous chloride, and the method of reacting nitric acid and sulfur dioxide. However, in general, in crude nitrogen monoxide gas, Contains moisture, acid gases such as nitrogen dioxide and sulfur dioxide as impurities or by-products. In particular, in the production of nitric oxide by reducing nitric acid with sulfur dioxide, sulfur dioxide is contained as an impurity in crude nitrogen monoxide. In order to form the above-mentioned oxynitride film in a semiconductor process, it is desirable that nitrogen monoxide as a material gas be of high purity. [0003] As a relat...

Claims

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Application Information

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IPC IPC(8): C01B21/24
CPCB01D53/02B01D53/1456B01D53/1481B01D2252/10B01D2253/10B01D2257/80C01B21/24
Inventor 川上纯一田井慎一横野孝尔
Owner SUMITOMO SEIKA CHEM CO LTD